CN106757245A - A kind of process of surface treatment of melanism Copper Foil - Google Patents

A kind of process of surface treatment of melanism Copper Foil Download PDF

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Publication number
CN106757245A
CN106757245A CN201611030607.XA CN201611030607A CN106757245A CN 106757245 A CN106757245 A CN 106757245A CN 201611030607 A CN201611030607 A CN 201611030607A CN 106757245 A CN106757245 A CN 106757245A
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copper foil
melanism
surface treatment
temperature
potassium
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CN106757245B (en
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王学江
王维河
杨祥魁
徐策
徐树民
刘建广
徐好强
冯秋兴
姜晓亮
朱义刚
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SHANDONG JINBAO ELECTRONICS CO Ltd
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SHANDONG JINBAO ELECTRONIC CO Ltd
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/06—Wires; Strips; Foils
    • C25D7/0614—Strips or foils
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34—Pretreatment of metallic surfaces to be electroplated

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Electroplating And Plating Baths Therefor (AREA)

Abstract

The present invention relates to a kind of process of surface treatment of melanism Copper Foil, using electrolytic copper foil or rolled copper foil as negative electrode, and constantly run forward, its typical process flow is：--- melanism --- dry, and the melanism Copper Foil that present invention process is prepared has good decay resistance and etching performance, while having excellent normal temperature, high-temperature oxidation resistance by anti-oxidation --- silane coupler --- for roughening.For the Copper Foil of roughness Rz≤5 μm, it is very suitable for making flexibility coat copper plate, high-frequency circuit board.

Description

A kind of process of surface treatment of melanism Copper Foil
Technical field
The present invention relates to a kind of process of surface treatment of Copper Foil, more particularly to a kind of process of surface treatment of melanism Copper Foil, Belong to the technical field of producing of Copper Foil.
Background technology
Copper Foil is one of primary raw material of PCB productions, and the difference according to manufacturing process is broadly divided into electrolytic copper foil and calendering Two kinds of Copper Foil.Rolled copper foil has larger advantage in aspect of performances such as elongation percentage, resist bending, flexible printed-circuit board in the past (FPC) use rolled copper foil manufacturer more.In recent years, with the raising of electrolytic copper foil production technology level, Japanese part copper Paper tinsel producer has developed the high-quality electrolytic copper foil that many moneys disclosure satisfy that FPC requirements.Due to Productive Technology of Electronlytical Copper-foil and price The advantage of aspect, electrolytic copper foil is more and more applied to FPC.
The performances such as the corrosion-resistant, anti-oxidant of copper foil surface coating, the High temperature diffusion of FPC must be in appropriate scope, no Can be too strong or excessively weak, the corrosion resistance of copper foil surface coating is stronger, occurs that etching is not net when PCB is etched online, makes highly dense Short circuit occurs during degree fine electronic circuit；Corrosion resistance is excessively weak, then lateral erosion occurs, occurs when making ultra-fine interval circuit Lines come off, and the antioxidant on surface is too strong, occur that microetch is not net in slim copper-clad plate or flexibility coat copper plate microetch, after influence The overlay film of sequence is made, and antioxidant is excessively weak, occurs that Copper Foil is aoxidized.Copper foil surface roughness is too small, and the consistency of Copper Foil is raised, The peel strength of the upper Copper Foils of FCCL declines, and resistance to bend(ing) is improved；Copper Foil roughness is excessive, and the compactness of Copper Foil declines, FCCL The peel strength of upper Copper Foil is raised, and resistance to bend(ing) declines, and when suppressing two-sided thin plate it is possible that back side pressure is worn and causes short Road.
China is to be only second to the second largest printed circuit board big export country after Japan, due to domestic top grade electrolytic copper foil There is larger gap in production technology, cause the situation that domestic high-rank copper foil relies primarily on import compared with the U.S., Japan, For high technology content and the FCCL Copper Foils of high added value, in numerous domestic production producers, there is no one can produce in batches, Most FCCL Copper Foils, are all from the area import such as Japan, South Korea, TaiWan, China.
Contain arsenic element in existing Copper Foil blackening treatment process, and arsenic element is classified as attention rate material high by REACH, belongs to 1st class carcinogen.Strict requirements are have to arsenogen as the component of product or product.
The technological difficulties of melanism Copper Foil production are the production of hair paper tinsel and black surface treatment of high-tensile, high-elongation Technology.
The content of the invention
A kind of deficiency that the present invention exists for existing Copper Foil production technology gained Copper Foil aspect of performance, there is provided melanism Copper Foil Process of surface treatment.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：
A kind of process of surface treatment of melanism Copper Foil, using electrolytic copper foil or rolled copper foil as electrode, and constantly forward Run, its typical process flow is：--- melanism --- dry, specifically by such as by anti-oxidation --- silane coupler --- for roughening Lower step：
1) it is roughened：Copper sulphate, nickel sulfate are dissolved in water, after be added thereto to sulfuric acid, it is well mixed after be and prepare Roughening solution, Copper Foil is placed in the roughening solution and is electroplated；
2) melanism：Additive, copper sulphate, zinc sulfate are dissolved in water respectively, the one or both in cobaltous sulfate, nickel sulfate Mixture be dissolved in water, after all solution are added in additive solution are well mixed and are stirred continuously, adjust pH value, Wherein control parameter is as follows：Cu2+5-20g/L, Zn2+2-10g/L, Co2+0-20g/L, Ni2+0-20g/L, while Co2+With Ni2+'s Concentration He≤1g/L, PH≤6.5, additive 5-80g/L, 25-50 DEG C of temperature, current density 5-20A/dm2, electroplating time 3- 15s；
3) it is anti-oxidation：Potassium chromate, zinc sulfate, potassium pyrophosphate are dissolved in water respectively, zinc sulfate, potassium chromate is slow respectively Add potassium pyrophosphate solution in and be stirred continuously, regulation pH value for alkalescence, the Copper Foil after Darkening process is placed in the mixed solution In electroplated；
4) silane coupler：Silane coupler is added to the water and is stirred, be applied to copper foil surface；
5) dry.
On the basis of above-mentioned technical proposal, the present invention can also do following improvement.
Further, step 1) control parameter is as follows：Cu2+16-40g/L, Ni2+5-10g/L, H2SO480-220g/L, temperature 20-40 DEG C, current density 20-50A/dm2, electroplating time 5-15s, being roughened can be roughened to the mat surface of electrolytic copper foil, also The wet look of Copper Foil can be roughened, it is therefore intended that improve peel strength of the Copper Foil in copper-clad plate.
Further, step 3) in control parameter it is as follows：Cr6+1.5-12g/L, Zn2+0.6-9g/L, K4P2O770-200g/L, PH 9-12,25-40 DEG C of temperature, current density 2-12A/dm2, electroplating time 1-5s, the anti-oxidation surface electricity being mainly in Copper Foil One layer of zinc-evanohm of plating, to improve normal temperature, the high-temperature oxidation resistance of Copper Foil.
Further, step 4) in control parameter it is as follows：Silane coupler 0.5-8g/L, 20-35 DEG C of temperature, process time 2- 5s, applies the purpose of silane coupler, on the one hand improves peel strength of the Copper Foil in copper-clad plate, on the other hand can also improve copper The normal temperature oxidation resistent susceptibility of paper tinsel.
Further, the silane coupler is γ-glycidyl ether oxygen propyl trimethoxy silicane, 3- aminopropyl front threes One or more mixture in TMOS, 3- aminopropyl triethoxysilanes.
Further, step 2) described in additive be tartaric acid, potassium tartrate, sodium tartrate, ammonium tartrate, potassium tartrate One or more in sodium, citric acid, potassium citrate, sodium citrate, ammonium citrate of mixture.
The beneficial effects of the invention are as follows：
1) the melanism Copper Foil prepared has good decay resistance and etching performance, at the same have excellent normal temperature, High-temperature oxidation resistance.The melanism Copper Foil for being prepared using this technique after tested deposits 24h under the conditions of 80 DEG C of temperature, humidity 90% Surface is without substantially oxidation point, while depositing 30min non-oxidation phenomenons at 200 DEG C.For the Copper Foil of roughness Rz≤5 μm, very It is suitable for making flexibility coat copper plate, high-frequency circuit board；
2) the harmful elements such as lead, mercury, chromium, arsenic are not used in blackening process, beneficial to environmental protection and operative employee People's is healthy；
3) production process of melanism Copper Foil is simplified, technique is simpler easy, operation more facilitates.
The present invention is also claimed the Copper Foil prepared using the process of surface treatment of above-mentioned melanism Copper Foil in flexibility Application in copper-clad plate, high-frequency circuit board or electromagnetic shielding film.
Brief description of the drawings
Fig. 1 is 12 μm of LP Copper Foil M faces SEM photographs without present invention process treatment；
Fig. 2 is through 12 μm of black Copper Foil M faces SEM photographs after the PROCESS FOR TREATMENT of embodiment 1；
Fig. 3 is 18 μm of LP Copper Foil M faces SEM photographs without present invention process treatment；
Fig. 4 is through 18 μm of LP Copper Foil M faces SEM photographs after the PROCESS FOR TREATMENT of embodiment 2.
Specific embodiment
Principle of the invention and feature are described below in conjunction with example, example is served only for explaining the present invention, and It is non-for limiting the scope of the present invention.
Embodiment 1：
A kind of process of surface treatment of melanism Copper Foil, it is electrode to use 12 μm of electrolytic copper foils, specifically by following steps：
1) it is roughened：Copper sulphate, nickel sulfate are dissolved in water, after be added thereto to sulfuric acid, it is well mixed after be and prepare Roughening solution, Copper Foil is placed in the roughening solution and is electroplated, control the technological parameter to be：Cu2+16g/L, Ni2+5g/L, H2SO4220g/L, 20 DEG C of temperature, current density 32A/dm2, electroplating time 15s；
2) melanism：Additive potassium tartrate, copper sulphate, zinc sulfate are dissolved in water respectively, cobaltous sulfate is dissolved in water, after will All solution are added in additive solution and are well mixed and are stirred continuously, and adjust pH value, and wherein control parameter is as follows：Cu2+ 7g/L, Zn2+4g/L, Co2+20g/L, PH 6.5, potassium tartrate 67g/L, 42 DEG C of temperature, current density 5A/dm2, electroplating time 10s；
3) it is anti-oxidation：Potassium chromate, zinc sulfate, potassium pyrophosphate are dissolved in water respectively, zinc sulfate, potassium chromate is slow respectively Add potassium pyrophosphate solution in and be stirred continuously, adjust pH value, the Copper Foil after Darkening process is placed in the mixed solution to be carried out Plating, wherein control parameter is as follows：Cr6+1.5g/L, Zn2+0.6g/L, K4P2O770g/L, pH 12,40 DEG C of temperature, current density 7A/dm2, electroplating time 2.8s；
4) silane coupler：Silane coupler γ-glycidyl ether oxygen propyl trimethoxy silicane is added to the water stirring Uniformly, copper foil surface is applied to, wherein control silane coupler 0.5g/L, 35 DEG C of temperature, process time 3s；
5) dry：180 DEG C of temperature, process time 5s.
Embodiment 2：
The present embodiment and the difference of embodiment 1 are that to use 18 μm of LP Copper Foils be electrode, the technique of each step State modulator is as follows：
1) it is roughened：Cu2+20g/L, Ni2+7g/L, H2SO4150g/L, 34 DEG C of temperature, current density 26A/dm2, electroplating time 8s。
2) melanism：Cu2+10g/L, Zn2+6g/L, Co2+8g/L, Ni2+8g/L, pH 5.0, tartaric acid 5g/L, 38 DEG C of temperature, Current density 12A/dm2, electroplating time 8s.
3) it is anti-oxidation：Cr6+3g/L, Zn2+3.5g/L, K4P2O7120g/L, PH 9.5,32 DEG C of temperature, current density 5A/ dm2, electroplating time 2s.
4) silane coupler：3- TSL 8330 2g/L, 30 DEG C of temperature, process time 3s.
5) dry：220 DEG C of temperature, process time 4s.
Embodiment 3：
The present embodiment is that the process parameter control of each step is as follows with the difference of embodiment 1：
1) it is roughened Cu2+26g/L, Ni2+8g/L, H2SO4120g/L, 36 DEG C of temperature, current density 20A/dm2, electroplating time 5s。
2) melanism：Cu2+20g/L, Zn2+10g/L, Co2+10g/L, Ni2+20g/L, PH 4.2, potassium citrate 10g/L, lemon Lemon acid ammonium 25g/L, 30 DEG C of temperature, current density 20A/dm2, electroplating time 12s.
3) it is anti-oxidation：Cr6+6g/L, Zn2+5g/L, K4P2O7155g/L, PH 9.2,29 DEG C of temperature, current density 10A/dm2, Electroplating time 1.6s.
4) silane coupler：3- aminopropyl triethoxysilane 3g/L, 26 DEG C of temperature, process time 4s.
5) dry：100 DEG C of temperature, process time 6s.
Embodiment 4：
The present embodiment is that the process parameter control of each step is as follows with the difference of embodiment 1：
1) it is roughened Cu2+40g/L, Ni2+10g/L, H2SO480g/L, 40 DEG C of temperature, current density 50A/dm2, electroplating time 10s；
2) melanism：Cu2+5g/L, Zn2+2g/L, Ni2+1g/L, PH 3.0, ammonium tartrate 80g/L, 43 DEG C of temperature, electric current is close Degree 12A/dm2, electroplating time 10s；
3) it is anti-oxidation：Cr6+12g/L, Zn2+9g/L, K4P2O7200g/L, PH 9,25 DEG C of temperature, current density 8A/dm2, electricity Plating time 3s；
4) silane coupler：3- aminopropyl triethoxysilanes 2g/L, 3- aminopropyl trimethoxysilane 6g/L, temperature 20 DEG C, process time 3s；
5) dry：280 DEG C of temperature, process time 3s.
Table 1：Embodiment 1-4 gained Copper Foil performance test datas
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all it is of the invention spirit and Within principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.

Claims (7)

1. a kind of process of surface treatment of melanism Copper Foil, it is characterised in that using electrolytic copper foil or rolled copper foil as electrode, and Constantly run forward, specifically by following steps：
1) it is roughened：Copper sulphate, nickel sulfate are dissolved in water, after be added thereto to sulfuric acid, it is well mixed after be prepare thick Change solution, Copper Foil is placed in the roughening solution and is electroplated；
2) melanism：Additive, copper sulphate, zinc sulfate are dissolved in water respectively, the one or both in cobaltous sulfate, nickel sulfate it is mixed Compound is dissolved in water, after all solution are added in additive solution are well mixed and are stirred continuously, adjust pH value, wherein Control parameter is as follows：Cu2+5-20g/L, Zn2+2-10g/L, Co2+0-20g/L, Ni2+0-20g/L, while Co2+With Ni2+Concentration He≤1g/L, PH≤6.5, additive 5-80g/L, 25-50 DEG C of temperature, current density 5-20A/dm2, electroplating time 3-15s；
3) it is anti-oxidation：Potassium chromate, zinc sulfate, potassium pyrophosphate are dissolved in water respectively, zinc sulfate, potassium chromate are respectively added slowly to In potassium pyrophosphate solution and it is stirred continuously, regulation pH value is alkalescence, and the Copper Foil after Darkening process is placed in the mixed solution Row plating；
4) silane coupler：Silane coupler is added to the water and is stirred, be applied to copper foil surface；
5) dry.
2. the process of surface treatment of melanism Copper Foil according to claim 1, it is characterised in that step 1) control parameter is such as Under：Cu2+16-40g/L, Ni2+5-10g/L, H2SO480-220g/L, 20-40 DEG C of temperature, current density 20-50A/dm2, plating Time 5-15s.
3. the process of surface treatment of melanism Copper Foil according to claim 1, it is characterised in that step 3) in control parameter such as Under：Cr6+1.5-12g/L, Zn2+0.6-9g/L, K4P2O770-200g/L, pH 9-12,25-40 DEG C of temperature, current density 2- 12A/dm2, electroplating time 1-5s.
4. the process of surface treatment of melanism Copper Foil according to claim 1, it is characterised in that step 4) in control parameter such as Under：Silane coupler 0.5-8g/L, 20-35 DEG C of temperature, process time 2-5s.
5. the process of surface treatment of melanism Copper Foil according to claim 1, it is characterised in that step 2) described in additive It is tartaric acid, potassium tartrate, sodium tartrate, ammonium tartrate, sodium potassium tartrate tetrahydrate, citric acid, potassium citrate, sodium citrate, lemon One or more in sour ammonium of mixture.
6. the process of surface treatment of melanism Copper Foil according to claim 1, it is characterised in that step 4) described in silane Coupling agent is γ-glycidyl ether oxygen propyl trimethoxy silicane, 3- TSL 8330s, the ethoxy of 3- aminopropyls three One or more mixture in base silane.
7. the Copper Foil that a kind of handling process as any one of claim 1-6 is prepared is in flexibility coat copper plate, high frequency Application in circuit board or electromagnetic shielding film.
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Cited By (14)

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Publication number Priority date Publication date Assignee Title
CN108085726A (en) * 2017-12-21 2018-05-29 上海理工大学 The surface Darkening process method of rolled copper foil
CN108588770A (en) * 2018-05-04 2018-09-28 瑞声科技(新加坡)有限公司 Roll copper darkening ring piece preparation method and calendering copper darkening ring piece
CN108668450A (en) * 2018-03-16 2018-10-16 深圳丹邦科技股份有限公司 A kind of adhesion without adhesiver dosage form flexible copper-clad plate and preparation method thereof
CN108677231A (en) * 2018-05-04 2018-10-19 瑞声科技(新加坡)有限公司 Roll copper darkening ring piece preparation method and calendering copper darkening ring piece
CN108754477A (en) * 2018-05-04 2018-11-06 瑞声科技(新加坡)有限公司 Roll copper darkening ring piece preparation method and calendering copper darkening ring piece
CN109234772A (en) * 2018-09-10 2019-01-18 南亚电子材料(昆山)有限公司 A kind of Zn-Cr antioxygen chemical plating solution preparation method and the application on lithium ion battery copper foil
CN110029391A (en) * 2019-03-28 2019-07-19 中国恩菲工程技术有限公司 Modified copper foil in surface and preparation method thereof
CN112011810A (en) * 2020-08-26 2020-12-01 九江德福科技股份有限公司 Production method of high-heat-resistance electrolytic copper foil
CN112068328A (en) * 2020-09-09 2020-12-11 温州市皓朗眼镜有限公司 Corrosion-resistant glasses frame and processing technology thereof
CN112962128A (en) * 2021-01-29 2021-06-15 山东金宝电子股份有限公司 Coarsening process method of high-peeling-resistance copper foil
CN113549965A (en) * 2021-07-30 2021-10-26 江苏铭丰电子材料科技有限公司 Electroplating blackening process for ultra-low profile copper foil
CN113594048A (en) * 2021-06-25 2021-11-02 广东华智芯电子科技有限公司 Copper lead frame and surface treatment method thereof, package and preparation method thereof
CN113737238A (en) * 2021-10-11 2021-12-03 中色奥博特铜铝业有限公司 Surface roughening treatment method for ultra-low profile rolled copper foil
CN116970934A (en) * 2023-08-03 2023-10-31 广东盈华电子科技有限公司 Double-sided blackening surface treatment process for electrolytic copper foil

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CN102418129A (en) * 2011-11-18 2012-04-18 山东金宝电子股份有限公司 Surface treatment process of copper foil for high-Tg halogen-free plate
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Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108085726A (en) * 2017-12-21 2018-05-29 上海理工大学 The surface Darkening process method of rolled copper foil
CN108668450A (en) * 2018-03-16 2018-10-16 深圳丹邦科技股份有限公司 A kind of adhesion without adhesiver dosage form flexible copper-clad plate and preparation method thereof
CN108668450B (en) * 2018-03-16 2020-09-29 深圳丹邦科技股份有限公司 Non-adhesive flexible copper clad laminate and preparation method thereof
CN108588770A (en) * 2018-05-04 2018-09-28 瑞声科技(新加坡)有限公司 Roll copper darkening ring piece preparation method and calendering copper darkening ring piece
CN108677231A (en) * 2018-05-04 2018-10-19 瑞声科技(新加坡)有限公司 Roll copper darkening ring piece preparation method and calendering copper darkening ring piece
CN108754477A (en) * 2018-05-04 2018-11-06 瑞声科技(新加坡)有限公司 Roll copper darkening ring piece preparation method and calendering copper darkening ring piece
CN109234772A (en) * 2018-09-10 2019-01-18 南亚电子材料(昆山)有限公司 A kind of Zn-Cr antioxygen chemical plating solution preparation method and the application on lithium ion battery copper foil
CN110029391A (en) * 2019-03-28 2019-07-19 中国恩菲工程技术有限公司 Modified copper foil in surface and preparation method thereof
CN112011810A (en) * 2020-08-26 2020-12-01 九江德福科技股份有限公司 Production method of high-heat-resistance electrolytic copper foil
CN112068328A (en) * 2020-09-09 2020-12-11 温州市皓朗眼镜有限公司 Corrosion-resistant glasses frame and processing technology thereof
CN112068328B (en) * 2020-09-09 2022-02-22 温州市皓朗眼镜有限公司 Corrosion-resistant glasses frame and processing technology thereof
CN112962128A (en) * 2021-01-29 2021-06-15 山东金宝电子股份有限公司 Coarsening process method of high-peeling-resistance copper foil
CN113594048A (en) * 2021-06-25 2021-11-02 广东华智芯电子科技有限公司 Copper lead frame and surface treatment method thereof, package and preparation method thereof
CN113594048B (en) * 2021-06-25 2022-03-11 广东华智芯电子科技有限公司 Copper lead frame and surface treatment method thereof, package and preparation method thereof
CN113549965A (en) * 2021-07-30 2021-10-26 江苏铭丰电子材料科技有限公司 Electroplating blackening process for ultra-low profile copper foil
CN113737238A (en) * 2021-10-11 2021-12-03 中色奥博特铜铝业有限公司 Surface roughening treatment method for ultra-low profile rolled copper foil
CN116970934A (en) * 2023-08-03 2023-10-31 广东盈华电子科技有限公司 Double-sided blackening surface treatment process for electrolytic copper foil
CN116970934B (en) * 2023-08-03 2024-02-06 广东盈华电子科技有限公司 Double-sided blackening surface treatment process for electrolytic copper foil

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